Fipronil em açúcar: otimização, validação e aplicação da extração sólido-líquido com partição a baixa temperatura

Abstract

Crystal sugar is one of the most consumed products throughout Brazil. This product is derived from sugarcane juice followed by various cooking processes. In sugarcane cultivation, various types of agricultural implements and chemical products such as pesticides are used. One of the most commonly used pesticides in the sugarcane cultivation process is fipronil. In the state of Goiás alone, over 198 tons of this active ingredient were used. Despite the various industrial processes involved in crystal sugar production, residues of fipronil can end up in the final product due to the physicochemical properties of fipronil. Therefore, this research aims to optimize and validate an analytical method capable of identifying and quantifying the active ingredient fipronil in samples of crystal sugar. The chosen method was solid-liquid extraction with low-temperature partitioning followed by high-performance liquid chromatography analysis. The chosen analytical method has shown excellent results in various matrix types for different active ingredients. After method validation, sugar samples were collected from businesses located in the municipalities of Itumbiara - GO and Bom Jesus - GO to verify if there is fipronil contamination in the analyzed samples. For method optimization, a 22 factorial design was employed, and it was possible to obtain fipronil recovery rates in the sugar matrix of 91.04%. To certify the method's reliability, certain parameters were evaluated, such as linearity, which resulted in a coefficient of determination (R2) above 0.99, a detection limit (LD) of 0.02 mg kg-1, and a quantification limit (LQ) of 0.07 mg kg-1. Considering the values obtained for these parameters, along with the relative standard deviation (RSD) within a range of less than 20%, it can be stated that the SLE-LTP method is precise and accurate, making it applicable for determining fipronil in sugar matrices.